CN203674160U - Sample feeding device for online mass spectrometer - Google Patents

Sample feeding device for online mass spectrometer Download PDF

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Publication number
CN203674160U
CN203674160U CN201320849995.XU CN201320849995U CN203674160U CN 203674160 U CN203674160 U CN 203674160U CN 201320849995 U CN201320849995 U CN 201320849995U CN 203674160 U CN203674160 U CN 203674160U
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China
Prior art keywords
sample
outlet
sample cavity
sampling device
communicated
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Expired - Lifetime
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CN201320849995.XU
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Chinese (zh)
Inventor
张进伟
冯红年
郑利武
任焱
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Focused Photonics Hangzhou Inc
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Focused Photonics Hangzhou Inc
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Abstract

The utility model provides a sample feeding device for an online mass spectrometer. The sample feeding device comprises a sample feeding pipeline, a sample feeding chamber, a capillary tube, heating modules, and a first pumping module. The sample feeding pipeline is provided with an inlet and an outlet. Two opposite ends of the sample feeding chamber respectively comprise a sample inlet and a sample outlet which are arranged in a same line. The sectional area of the sample inlet is more than that of the sample outlet. The sample inlet is communicated with the interior of the sample feeding pipeline. The sample outlet is communicated with a vacuum chamber of the online mass spectrometer. The capillary tube is provided with two openings on the two ends thereof and is disposed inside the sample feeding chamber. An inlet end of the capillary tube is connected with one end, provided with the sample inlet, of the sample feeding chamber. The distance between an outlet end of the capillary tube and one end, provided with the sample outlet, of the sample feeding chamber is more than zero. The sample inlet and the sample outlet are arranged in an axial projection area of the capillary tube. The distance between the outer wall of the capillary tube and the inner wall of the sample feeding chamber is more than zero. The heating modules are used for heating the sample feeding chamber. The input end of a first pumping module is communicated with the side portion of the sample feeding chamber and the output end of the first pumping module is not connected. The sample feeding device for an online mass spectrometer has good adaptability.

Description

The sampling device of on-line mass spectroscopy analyzer
Technical field
The utility model relates to mass spectrometer, particularly the sampling device of on-line mass spectroscopy analyzer.
Background technology
On-line mass spectroscopy separates and detects according to different material mass-to-charge ratio difference, completes the analysis to measured matter.For reaching best detection effect, all separation and testing processes all complete in vacuum system, so require vacuum system to possess several conditions:
1, long-term stability maintains higher vacuum degree, conventionally below 1E-5Torr;
2, vacuum chamber system is difficult for polluting, and ambient noise signal is stable;
3, the sample gas pressure that enters vacuum chamber inside is stablized;
Fig. 1 has schematically provided vacuum decompression system of the prior art, as shown in Figure 1, uses 1/16 capillary 12 to be communicated with vacuum chamber 31 and sample channel 11, and adapter 13 is set between described capillary and sample channel; Use the combination of turbomolecular pump 32, diaphragm pump 34 to go to maintain the vacuum degree of vacuum chamber.Described depressurized system is more applicable in most of occasions, but higher to tested gas working condition requirement, must be by below secondary filter 0.1 μ m.Above-mentioned vacuum decompression system has many deficiencies, as:
1, capillary inner diameter less (25 μ m are following), and length is grown (more than 50mm).Contain easy condensed material if measured in background component, capillary is easy to blocked due to absorption, even pollutes vacuum cavity, causes ambient noise signal fluctuation, thereby causing to measure is forbidden;
2, in the time that sample atmospheric pressure has larger fluctuation, can cause fluctuation vacuum, even cause and enter the inner sample throughput fluctuation of vacuum chamber, make sample gas signal produce surging, finally cause to measure and forbidden, or abnormal crest occurs;
3, dust and drop easily enter mass spectrum vacuum chamber inside and cause vacuum cavity contaminated;
4, need to use accurate filter, improve cost.
Utility model content
In order to solve the deficiency in above-mentioned prior art scheme, the utility model provides a kind of simple in structure, adaptable, sampling device of on-line mass spectroscopy analyzer cheaply.
The purpose of this utility model is achieved through the following technical solutions:
A sampling device for on-line mass spectroscopy analyzer, described sampling device comprise there is entrance, the sample channel of drain; Described sampling device further comprises:
Sample cavity, the relative two ends of described sample cavity have respectively injection port, the outlet of conllinear, and the sectional area of described injection port is greater than described outlet; Described injection port is communicated with the inside of described pipeline, and described outlet is communicated with the vacuum chamber of described on-line mass spectroscopy analyzer;
Capillary, described capillary both ends open is also arranged in described sample cavity, and one end with injection port of entrance point and described sample cavity is connected, and the distance that the port of export and described sample cavity have one end of outlet is greater than zero; Described injection port and sample outlet position are in described axis projection capillaceous region; The spacing of the inwall of described outer wall capillaceous and sample cavity is greater than zero;
Heating module, described heating module is used for heating described sample cavity;
The first suction module, the input of described the first suction module is communicated with the sidepiece of described sample cavity, output emptying.
According to above-mentioned sampling device, preferably, the diameter of described injection port is 100-150 μ m.
According to above-mentioned sampling device, preferably, the diameter of described outlet is 25-50 μ m.
According to above-mentioned sampling device, preferably, described the first suction module adopts mechanical pump.
According to above-mentioned sampling device, preferably, described specification capillaceous is 1/8.
According to above-mentioned sampling device, preferably, described vacuum chamber is communicated with the second suction module, and described suction module comprises:
Be communicated with successively turbomolecular pump, oil mist trapping device and mechanical pump.
Compared with prior art, the beneficial effect the utlity model has is:
1, being designed with of sample cavity helps increase internal diameter capillaceous, effectively prevented obstruction capillaceous; The larger volume of sample cavity has prevented the fluctuation of sample atmospheric pressure and sample throughput fluctuation in the vacuum chamber that brings, has avoided the appearance of the fluctuation problem of measuring-signal;
2, the design of heating module has prevented the easily condensation of condensed material in sample gas, the first suction module is extracted out sample cavity such as impurity, drop etc. in sample gas, effectively prevent the pollution with capillary, vacuum chamber, avoid the appearance of the unstable problem of ambient noise signal, strengthen the contamination resistance of vacuum chamber, extended the maintenance period of on-line mass spectroscopy analyzer;
3, the setting of oil mist trapping device has prevented contaminated with oil mist molecular pump, the vacuum chamber that mechanical pump produces;
4, without being equipped with accurate filter.
Brief description of the drawings
With reference to accompanying drawing, disclosure of the present utility model will be easier to understand.Those skilled in the art hold intelligible: these accompanying drawings are only for illustrating the technical solution of the utility model, and are not intended to protection range of the present utility model to be construed as limiting.In figure:
Fig. 1 is according to the structure diagram of vacuum decompression system in the prior art of the utility model embodiment 1;
Fig. 2 is according to the structure diagram of the sampling device of the utility model embodiment 1;
Fig. 3 is the course of work flow chart according to the sampling device of the utility model embodiment 1.
Embodiment
Fig. 2,3 and following declarative description optional execution mode of the present utility model how to implement and to reproduce the utility model with instruction those skilled in the art.In order to instruct technical solutions of the utility model, simplify or omitted some conventional aspects.Those skilled in the art should understand that be derived from these execution modes modification or replace will be in scope of the present utility model.Those skilled in the art should understand that following characteristics can combine to form multiple modification of the present utility model in every way.Thus, the utility model is not limited to following optional execution mode, and is only limited by claim and their equivalent.
Embodiment 1:
Fig. 2 has schematically provided the structure diagram of the sampling device of the on-line mass spectroscopy analyzer of the utility model embodiment, and as shown in Figure 2, described sampling device comprises:
Sample channel 11, described sample channel has entrance, drain; The concrete structure of described sample channel and material are the state of the art, do not repeat them here;
Sample cavity 21, the relative two ends of described sample cavity 21 have respectively the injection port 23 of conllinear, outlet 24, and the sectional area of described injection port 23 is greater than described outlet 24; Described injection port 23 is communicated with the inside of described pipeline 11, and described outlet 24 is communicated with the vacuum chamber 32 of described on-line mass spectroscopy analyzer; Preferably, the diameter of described injection port 23 is 100-150 μ m, and the diameter of described outlet 24 is 25-50 μ m;
Capillary 22, described capillary 22 both ends opens are also arranged in described sample cavity 21, and one end with injection port 23 of entrance point and described sample cavity 21 is connected, and the distance that the port of export and described sample cavity 21 have one end of outlet 24 is greater than zero; In described injection port 23 and the outlet 24 axis projection region in described capillary 22; The spacing of the inwall of the outer wall of described capillary 22 and sample cavity 21 is greater than zero;
Heating module 25, described heating module 25, for heating described sample cavity, prevents the condensation of the part composition in the interior sample gas of sample cavity 21; Described heating module 25 is arranged on the periphery of sample cavity 21, can adopt the mode such as electric heating, steam tracing;
The first suction module, the input of described the first suction module is communicated with the sidepiece of described sample cavity, output emptying.Preferably, described the first suction module comprises adjuster valve 26, mechanical pump 27.
In order to maintain the vacuum degree of vacuum chamber 31, described vacuum chamber 31 is communicated with the second suction module, and described suction module comprises:
The turbomolecular pump 32, oil mist trapping device 33 and the mechanical pump 34 that connect successively.
Fig. 3 has schematically provided the course of work of the sampling device of above-mentioned on-line mass spectroscopy analyzer, and (arrow represents gas flow direction) as shown in Figure 3, the described course of work comprises the following steps:
(A1) sample cavity and vacuum chamber maintain certain vacuum degree;
(A2) sample gas is by described sample channel, and most of emptying from evacuation port, fraction enters in sample cavity from injection port;
(A3) the sample gas that enters described sample cavity is from inner outflow capillaceous, and fraction enters vacuum chamber from outlet, and major part enters sample cavity and intercapillary region, is extracted out described sample cavity emptying afterwards by the first suction module;
In above-mentioned work, heating module heating sample cavity, prevents that part composition condensation in sample gas is in capillary.
In order to maintain the vacuum degree of sample cavity and vacuum chamber, alternatively, (A1) is further comprising the steps for step:
(B1) mechanical pump that is communicated with respectively described sample cavity, vacuum chamber is opened;
(B2) the turbo-molecular pump work between described vacuum chamber and mechanical pump;
In the above-mentioned process vacuumizing, the oil mist trapping device being arranged between turbomolecular pump and mechanical pump starts, the mist of oil that Capturing machine pump produces.
The benefit reaching according to the sampling device of the utility model embodiment 1 and method of work thereof is: the design of sample cavity and the first suction module, improve internal diameter capillaceous on the one hand, and effectively prevent obstruction; Can extract out sample cavity such as drop, impurity etc. in sample gas in time on the other hand, prevent from entering vacuum chamber, without being equipped with accurate filter; On the one hand, the sample cavity of larger volume has reduced the impact that sample throughput fluctuates on sample throughput in vacuum chamber again.The design of heating module prevented some composition condensation in capillary in sample gas, ensured mobile unobstructed in capillary of sample gas.
Embodiment 2:
According to the sampling device of on-line mass spectroscopy analyzer of the utility model embodiment 1 and the application examples of method of work.
In this application examples, sample cavity adopts cylindrical structure, and internal diameter is 10mm, Cylindorical rod to the two ends of sealing be respectively equipped with coaxial sample holes, sample outlet hole, the diameter of described sample holes is 120 μ m, the diameter of sample outlet hole is 35 μ m.Capillary inner diameter is 75 μ m (being greater than the internal diameter capillaceous using in prior art), be arranged in described sample cavity, one end is connected with the blind end with sample holes, the other end maintains a certain distance with the blind end with sample outlet hole, as 5mm, described capillary and described sample holes, sample outlet hole are coaxial.Described sample holes, sample outlet hole are in described axis projection capillaceous region.Distance between outer wall capillaceous and the inwall of sample cavity is greater than zero.Described sample holes is communicated with respectively sample channel, sample cavity, and described sample outlet hole is communicated with respectively vacuum chamber, sample cavity.The first suction module comprises diaphragm pump, and described diaphragm pump is connected to the sidepiece of described sample cavity by valve, with sample cavity internal communication.Heating module adopts electric heater, is arranged on the periphery of sample cavity.
Vacuum chamber is communicated with the second suction module, specifically be communicated with successively turbomolecular pump, diaphragm pump, in order to prevent that the mist of oil of diaphragm pump from entering in vacuum chamber, oil mist trapping device is set between turbomolecular pump and diaphragm pump, prevent contaminated with oil mist molecular pump, vacuum chamber that diaphragm pump produces.
The modus operandi of above-mentioned sampling device is specially:
(A1) diaphragm pump that is communicated with respectively described sample cavity, vacuum chamber is opened; While reaching below 4Torr with the vacuum degree in vacuum chamber, open the turbomolecular pump between described vacuum chamber and mechanical pump;
In said process, the oil mist trapping device being arranged between turbomolecular pump and diaphragm pump is opened, the mist of oil that trapping diaphragm pump produces;
(A2) sample gas is by described sample channel, and most of emptying from evacuation port, fraction enters in capillary from sample holes;
(A3) sample gas flows out in capillary, and fraction enters vacuum chamber from outlet, and major part enters sample cavity and intercapillary region, is extracted out described sample cavity emptying afterwards by the first suction module;
In above-mentioned work, heating module heating sample cavity, prevents that composition condensation in sample gas is in capillary.
Embodiment 3:
According to the sampling device of on-line mass spectroscopy analyzer of the utility model embodiment 1 and the application examples of method of work.
In this application examples, sample cavity adopts cylindrical structure, and internal diameter is 12mm, Cylindorical rod to the two ends of sealing be respectively equipped with coaxial sample holes, sample outlet hole, the diameter of described sample holes is 150 μ m, the diameter of sample outlet hole is 50 μ m.Capillary inner diameter is 50 μ m (being greater than the internal diameter capillaceous using in prior art), be arranged in described sample cavity, one end is connected with the blind end with sample holes, the other end maintains a certain distance with the blind end with sample outlet hole, as 3mm, described capillary and described sample holes, sample outlet hole are coaxial.Described sample holes, sample outlet hole are in described axis projection capillaceous region.Distance between outer wall capillaceous and the inwall of sample cavity is greater than zero.Described sample holes is communicated with respectively sample channel, sample cavity, and described sample outlet hole is communicated with respectively vacuum chamber, sample cavity.The first suction module comprises diaphragm pump, and described diaphragm pump is connected to the sidepiece of described sample cavity by valve, with sample cavity internal communication.
Vacuum chamber is communicated with the second suction module, is specifically communicated with successively turbomolecular pump, diaphragm pump, in order to prevent that the mist of oil of diaphragm pump from entering in vacuum chamber, arranges oil mist trapping device between turbomolecular pump and diaphragm pump.
Above-described embodiment is only the size that has exemplarily provided injection port, outlet, can also be other size certainly, and if injection port diameter is 100 μ m, outlet diameter is 25 μ m.

Claims (6)

1. a sampling device for on-line mass spectroscopy analyzer, described sampling device comprise there is entrance, the sample channel of drain; It is characterized in that: described sampling device further comprises:
Sample cavity, the relative two ends of described sample cavity have respectively injection port, the outlet of conllinear, and the sectional area of described injection port is greater than described outlet; Described injection port is communicated with the inside of described pipeline, and described outlet is communicated with the vacuum chamber of described on-line mass spectroscopy analyzer;
Capillary, described capillary both ends open is also arranged in described sample cavity, and one end with injection port of entrance point and described sample cavity is connected, and the distance that the port of export and described sample cavity have one end of outlet is greater than zero; Described injection port and sample outlet position are in described axis projection capillaceous region; The spacing of the inwall of described outer wall capillaceous and sample cavity is greater than zero;
Heating module, described heating module is used for heating described sample cavity;
The first suction module, the input of described the first suction module is communicated with the sidepiece of described sample cavity, output emptying.
2. sampling device according to claim 1, is characterized in that: the diameter of described injection port is 100-150 μ m.
3. sampling device according to claim 1, is characterized in that: the diameter of described outlet is 25-50 μ m.
4. sampling device according to claim 1, is characterized in that: described the first suction module adopts mechanical pump.
5. sampling device according to claim 1, is characterized in that: described specification capillaceous is 1/8.
6. sampling device according to claim 1, is characterized in that: described vacuum chamber is communicated with the second suction module, and described suction module comprises:
Be communicated with successively turbomolecular pump, oil mist trapping device and mechanical pump.
CN201320849995.XU 2013-12-13 2013-12-13 Sample feeding device for online mass spectrometer Expired - Lifetime CN203674160U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103681203A (en) * 2013-12-13 2014-03-26 聚光科技(杭州)股份有限公司 Sample device of online mass spectrum analyzer and working method thereof
CN113270308A (en) * 2021-05-20 2021-08-17 中国科学院工程热物理研究所 Sampling sleeve capable of preventing dust and removing dust, mass spectrum sampling interface and mass spectrum sampling method
CN115901350A (en) * 2021-08-04 2023-04-04 上海海珊智能仪器有限公司 Vacuum sampling fast online detection mass spectrometer system

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103681203A (en) * 2013-12-13 2014-03-26 聚光科技(杭州)股份有限公司 Sample device of online mass spectrum analyzer and working method thereof
CN113270308A (en) * 2021-05-20 2021-08-17 中国科学院工程热物理研究所 Sampling sleeve capable of preventing dust and removing dust, mass spectrum sampling interface and mass spectrum sampling method
CN113270308B (en) * 2021-05-20 2024-03-12 中国科学院工程热物理研究所 Sampling sleeve capable of preventing dust and removing dust, mass spectrum sampling interface and mass spectrum sampling method
CN115901350A (en) * 2021-08-04 2023-04-04 上海海珊智能仪器有限公司 Vacuum sampling fast online detection mass spectrometer system

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Granted publication date: 20140625

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